CN108475749A - Lithium rechargeable battery heat-sensitive layer - Google Patents
Lithium rechargeable battery heat-sensitive layer Download PDFInfo
- Publication number
- CN108475749A CN108475749A CN201680074455.5A CN201680074455A CN108475749A CN 108475749 A CN108475749 A CN 108475749A CN 201680074455 A CN201680074455 A CN 201680074455A CN 108475749 A CN108475749 A CN 108475749A
- Authority
- CN
- China
- Prior art keywords
- sensitive layer
- temperature
- component
- rechargeable battery
- heat
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
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- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 59
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- 238000013021 overheating Methods 0.000 abstract description 4
- 239000010410 layer Substances 0.000 description 230
- 125000006850 spacer group Chemical group 0.000 description 40
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 18
- -1 N-BMA Chemical compound 0.000 description 18
- 229910001416 lithium ion Inorganic materials 0.000 description 18
- 230000006978 adaptation Effects 0.000 description 16
- 238000010438 heat treatment Methods 0.000 description 16
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- FZYCEURIEDTWNS-UHFFFAOYSA-N prop-1-en-2-ylbenzene Chemical compound CC(=C)C1=CC=CC=C1.CC(=C)C1=CC=CC=C1 FZYCEURIEDTWNS-UHFFFAOYSA-N 0.000 description 1
- HJWLCRVIBGQPNF-UHFFFAOYSA-N prop-2-enylbenzene Chemical compound C=CCC1=CC=CC=C1 HJWLCRVIBGQPNF-UHFFFAOYSA-N 0.000 description 1
- BOQSSGDQNWEFSX-UHFFFAOYSA-N propan-2-yl 2-methylprop-2-enoate Chemical compound CC(C)OC(=O)C(C)=C BOQSSGDQNWEFSX-UHFFFAOYSA-N 0.000 description 1
- LYBIZMNPXTXVMV-UHFFFAOYSA-N propan-2-yl prop-2-enoate Chemical compound CC(C)OC(=O)C=C LYBIZMNPXTXVMV-UHFFFAOYSA-N 0.000 description 1
- NHARPDSAXCBDDR-UHFFFAOYSA-N propyl 2-methylprop-2-enoate Chemical compound CCCOC(=O)C(C)=C NHARPDSAXCBDDR-UHFFFAOYSA-N 0.000 description 1
- KOUKXHPPRFNWPP-UHFFFAOYSA-N pyrazine-2,5-dicarboxylic acid;hydrate Chemical group O.OC(=O)C1=CN=C(C(O)=O)C=N1 KOUKXHPPRFNWPP-UHFFFAOYSA-N 0.000 description 1
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- ZDQYSKICYIVCPN-UHFFFAOYSA-L sodium succinate (anhydrous) Chemical compound [Na+].[Na+].[O-]C(=O)CCC([O-])=O ZDQYSKICYIVCPN-UHFFFAOYSA-L 0.000 description 1
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- SJMYWORNLPSJQO-UHFFFAOYSA-N tert-butyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OC(C)(C)C SJMYWORNLPSJQO-UHFFFAOYSA-N 0.000 description 1
- 150000003866 tertiary ammonium salts Chemical class 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 125000003698 tetramethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 125000000383 tetramethylene group Chemical class [H]C([H])([*:1])C([H])([H])C([H])([H])C([H])([H])[*:2] 0.000 description 1
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- NJRXVEJTAYWCQJ-UHFFFAOYSA-N thiomalic acid Chemical compound OC(=O)CC(S)C(O)=O NJRXVEJTAYWCQJ-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/058—Construction or manufacture
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/411—Organic material
- H01M50/414—Synthetic resins, e.g. thermoplastics or thermosetting resins
- H01M50/417—Polyolefins
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
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Abstract
The purpose of the present invention is to provide the lithium rechargeable battery heat-sensitive layers that temperature rise is effectively hindered by making the resistance of inside battery increase when overheating extremely electric current is made to reduce.The lithium rechargeable battery of the present invention is formed with heat-sensitive layer by temperature-sensitive layer composition, the temperature-sensitive layer composition is located at particle made of the outside of the particle formed by the 1st component comprising the 2nd component substantial portion, the storage modulus of above-mentioned temperature-sensitive layer composition at 60 DEG C is 10kPa or more, and the storage modulus of above-mentioned temperature-sensitive layer composition at 150 DEG C is 1kPa or less.
Description
Technical field
The present invention relates to lithium rechargeable battery heat-sensitive layers.
Background technology
About small-sized, light weight and energy density height, the lithium rechargeable battery that can be repeatedly charged and discharged, from environment influence
Viewpoint is set out, it is contemplated that the expansion of its needs from now on.Lithium rechargeable battery energy density is high, is used in mobile phone, notes
The fields such as this computer, but along with the expansion of purposes, development, it is desirable that the further performance such as low resistance, high capacity carries
It is high.
Here, spacer is responsible for the critical function of the electric short circuit for the positive electrode and negative electrode for preventing lithium rechargeable battery.And
And as the spacer of lithium rechargeable battery, usually using the microporous membrane for example formed by polyolefin-based resins.In addition,
Spacer usually in the case where the temperature of inside battery becomes the high temperature near such as 130 DEG C, is blocked micro- porous by melting
To prevent the movement of lithium ion, the closing function for blocking electric current is played, is thus also responsible for and keeps lithium rechargeable battery
The effect of safety.However, work as causes battery temperature to further exceed the molten of the resin for constituting spacer because of the fever of moment
When point, spacer is drastically shunk sometimes, and positive electrode and negative electrode are in direct contact, and short-circuit position can expand.In this case, sometimes
Battery temperature rises to hundreds of DEG C or more, and battery reaches the state overheated extremely.
Here, temperature rise when being overheated to inhibit abnormal, proposes the micro-capsule using thermal expansivity.In patent document 1
In disclose a kind of collector, with resin layer and conductive adhesive linkage, used comprising thermoplastic in adhesive linkage
Thermal expansivity micro-capsule made of interior packet expanding material in the shell of property high molecular material.In addition, in patent document 2, making altogether
Thermal expansivity micro-capsule made of interior packet lower boiling hydrocarbons is dispersed in electrode active material layer in the shell of polymers.In turn, special
In sharp document 3, into electrolyte addition in the thermoplastic resins such as vinylidene chloride, acrylonitrile in-situ polymerization low boiling hydrocarbon,
The thermal expansivity micro-capsule of foaming agent.
Existing technical literature
Patent document
Patent document 1：No. 5177301 bulletins of Japanese Patent No.；
Patent document 2：No. 4929540 bulletins of Japanese Patent No.；
Patent document 3：Japanese Unexamined Patent Publication 2009-26674 bulletins.
Invention content
Problems to be solved by the invention
But in the micro-capsule of the thermal expansivity recorded in Patent Documents 1 to 3, the material using outside (shell) is needed
The material of inside is coating, for the material of complete coating inside, need the material in the outside using the amount of full.In turn, exist
In patent document 1, temperature rise when being overheated to inhibit abnormal needs to make special collector, also, in patent document 2
In, binding material etc. must also be used in addition to the micro-capsule of thermal expansivity when forming electrode active material layer, it is inefficient.
Here, the purpose of the present invention is to provide a kind of lithium rechargeable battery heat-sensitive layers, by abnormal overheat
When make inside battery resistance rise so as to make electric current reduce and effectively hinder temperature rise.
The solution to the problem
Present inventor has performed further investigations, as a result, it has been found that by using the temperature-sensitive layer composition comprising defined particle from
And can realize above-mentioned purpose, it has been finally completed the present invention.
That is, according to the present invention can provide,
(1) a kind of lithium rechargeable battery heat-sensitive layer, is formed by temperature-sensitive layer composition, and above-mentioned temperature-sensitive layer composition includes
2nd component substantial portion it is located at particle made of the outside of the particle formed by the 1st component, above-mentioned heat-sensitive layer at 60 DEG C
The storage modulus of composition be 10kPa or more, 150 DEG C of above-mentioned temperature-sensitive layer compositions storage modulus be 1kPa hereinafter,
(2) it according to the lithium rechargeable battery heat-sensitive layer described in (1), configures in positive active material opposite one another
Between layer and negative electrode active material layer,
(3) according to the lithium rechargeable battery heat-sensitive layer described in (1) or (2), the fusing point of above-mentioned 1st component be 60 DEG C with
It is upper and 160 DEG C hereinafter,
(4) the lithium rechargeable battery heat-sensitive layer according to any one of (1)~(3), the glass of above-mentioned 2nd component
Change transition temperature be -60 DEG C or more and 20 DEG C hereinafter,
(5) the lithium rechargeable battery heat-sensitive layer according to any one of (1)~(4), above-mentioned 1st component include number
Average molecular weight is 5000 or more and 15000 polyolefin below,
(6) a kind of lithium rechargeable battery, between the positive electrode active material layer and the negative electrode active material layer opposite one another
With the lithium rechargeable battery heat-sensitive layer according to any one of (1)~(5).
Invention effect
Lithium rechargeable battery heat-sensitive layer according to the present invention, by making on the resistance of inside battery when overheating extremely
It rises, effectively hinders temperature rise so as to make electric current reduce.
Specific implementation mode
Hereinafter, being illustrated with heat-sensitive layer to the lithium rechargeable battery of the present invention.The lithium rechargeable battery of the present invention
With heat-sensitive layer (hereinafter sometimes referred to " heat-sensitive layer ".) formed by temperature-sensitive layer composition, above-mentioned temperature-sensitive layer composition includes the 2nd component
It is located at particle made of the outside of the particle formed by the 1st component to substantial portion.Moreover, the 60 of above-mentioned temperature-sensitive layer composition
DEG C when storage modulus be 10kPa or more, storage modulus at 150 DEG C is 1kPa or less.
(temperature-sensitive layer composition)
The temperature-sensitive layer composition used in the present invention is located at comprising the 2nd component substantial portion to be formed by the 1st component
Particle made of the outside of particle is (hereinafter sometimes referred to simply as " particle ".).In addition, temperature-sensitive layer composition, which can contain, removes the 2nd group
The ingredient being located at dividing substantial portion other than particle made of the outside of the particle formed by the 1st component, but preferably only by this
Particle is constituted.
(particle)
Above-mentioned particle be the 2nd component substantial portion be located at made of the outside of the particle formed by the 1st component.
This, " be located to substantial portion ... and form " refers to that the particle that is formed by the 1st component is completely coating not by the 2nd component, grain
Expose the state for having the 1st component and the 2nd component in the surface of son.As such structure, can enumerate for example：As spherical grain
Son is formed by nucleocapsid knot from shell (the 2nd component) in central part (particle formed by the 1st component) by different polymer
In structure, the snowman's knot for the structure that the part of central part (particle formed by the 1st component) is exposed in shell (the 2nd component)
Structure；It is integrated in the particle (the 2nd component) of the other types of surface inserting of spherical particle (particle formed by the 1st component)
The octopus spline structure of structure etc..In addition, for particle, can by 2 kinds in various out-phase structure as described above with
On be further combined and form a compound particle.
In addition, as long as the particle at least surface layer part formed by the 1st component is constituted with the 1st component.That is, by the 1st
Component formed particle can be only made of the 1st component, can also the inside for the surface part being made of the 1st component contain with
The different other ingredients of 1st component.
(particle formed by the 1st component)
It is preferably molten when lithium rechargeable battery overheats extremely as the 1st component for constituting the particle formed by the 1st component
Viscosity when melting, melting becomes the ingredient of defined range, wherein particularly preferably using polymer such as polyolefin.
Here, polyolefin refers to the repetition for coming from the unsaturated hydrocarbons in the molecule with 1 or more carbon double bond
The polymer of unit (monomeric unit).Moreover, can be enumerated as polyolefin：High density polyethylene (HDPE), low density polyethylene (LDPE), poly- third
Alkene (PP), polybutene, polybutadiene, butadiene isoprene copolymer, polyisoprene, ethylene-vinyl acetate copolymer
(EVA), ethylene-ethyl acrylate copolymer, ethylene-propylene copolymer (EPR), ethylene-propylene-diene terpolymer, benzene
The hydride etc. of ethylene-butadiene block copolymer.These can respectively be used alone, or two or more is applied in combination.Separately
Outside, polyolefin can be used as the polyolefin derivatives such as chloridized polyolefin object.In addition, polyolefin can as polyolefin-wax and
It uses.In turn, the repetitive unit of the unsaturated hydrocarbons in the molecule with 1 or more carbon double bond is come from contained in polyolefin
The ratio of (monomeric unit) is preferably 70 mass % or more.
It is able to fully improve in lithium rechargeable battery from fusing point with the balancing good of viscosity when melting, in melting
From the perspective of resistance, the molecular weight of polyolefin is preferably 5000 or more, more preferably 6000 or more, further preferably 7000 with
On, preferably 15000 hereinafter, more preferably 12000 hereinafter, further preferably 10000 or less.When the molecular weight of polyolefin exists
When below the upper limit value of above range, viscosity when can inhibit due to melting is got higher, the polyolefin that melts becomes difficult to sprawl
And the phenomenon that fully internal resistance cannot being made to increase.In addition, when the molecular weight of polyolefin is more than the lower limiting value of above range, it can
Inhibit the phenomenon that the fusing point of polyolefin becomes too low.Therefore, even if do not overheat extremely it is usual in the state of can press down
The phenomenon that system causes internal resistance rising, battery performance to be remarkably decreased because of the melting of polyolefin.
So that the resistance of inside battery is increased from by the melting when overheating extremely, hinders temperature to make electric current reduce
From the perspective of rising, the fusing point of the 1st component is preferably 60 DEG C or more, more preferably 80 DEG C or more, preferably 160 DEG C hereinafter,
More preferably 140 DEG C or less.When the fusing point of the 1st component is in above range, can inhibit since fusing point is exceedingly high,
1st component melts front spacer is heat-shrinked and there is a phenomenon where short circuit, temperature to steeply rise.Furthermore it is possible to inhibit due to fusing point
It is exceedingly low therefore even if do not overheat extremely it is usual in the state of, caused due to the melting of the 1st component internal resistance rise,
The phenomenon that battery performance is remarkably decreased.
In addition, in the particle formed by the 1st component, it can further include and be added in the polymer such as polyolefin
Well known various additives (antioxidant).
(the 2nd component)
It is located at the 2nd component in the outside of the particle formed by the 1st component as substantial portion, as long as grain can be assigned
Sub- cohesive force is not particularly limited, it is preferable to use polymer such as acrylic acid series polymeric compounds.
In addition, the 2nd component usually has the composition different from the 1st component.
Acrylic acid series polymeric compounds are poly- comprising the monomeric unit that (methyl) acrylate compounds are polymerized
Close object.As acrylic acid series polymeric compounds, homopolymer, (methyl) acrylate chemical combination of (methyl) acrylate compounds can be enumerated
The copolymer etc. of object and the monomer that can be copolymerized with (methyl) acrylate compounds.By using (methyl) acrylate chemical combination
The polymer of object, so as to improve the heat-sensitive layer obtained based on the temperature-sensitive layer composition comprising particle to electrode active material layer
The adaptation of (positive electrode active material layer or negative electrode active material layer), spacer.In addition, in the present invention, " (methyl) propylene
Acid " means acrylic or methacrylic acid.
As (methyl) acrylate compounds, can enumerate for example：Methyl acrylate, ethyl acrylate, acrylic acid positive third
Ester, isopropyl acrylate, n-butyl acrylate, tert-butyl acrylate, amyl acrylate, Hexyl 2-propenoate, heptylacrylate, third
Olefin(e) acid monooctyl ester, acrylic acid nonyl ester, decyl acrylate, lauryl acrylate, n-myristyl base ester, stearyl acrylate,
The alkyl acrylates such as acrylic acid-2-ethyl caproite；The propylene such as acrylic acid -2- methoxy acrylates, acrylic acid -2- ethoxy ethyl esters
Sour alkoxy alkyl；Acrylic acid-the 2- such as acrylic acid -2- (perfluoro butyl) ethyl ester, acrylic acid -2- (perfluoropentyl) ethyl ester are (complete
Fluoroalkyl) ethyl ester；Methyl methacrylate, ethyl methacrylate, n propyl methacrylate, isopropyl methacrylate,
N-BMA, Tert-butyl Methacrylate, pentylmethacrylate, hexyl methacrylate, methacrylic acid heptan
Ester, 2-Propenoic acid, 2-methyl-, octyl ester, nonyl methacrylate, decyl-octyl methacrylate, lauryl methacrylate, methacrylic acid ten
The first such as trialkyl ester, methacrylic acid n-tetradecane base ester, stearyl methacrylate, methacrylic acid -2- ethylhexyls
Base alkyl acrylate；The methacrylic acids alkane such as methacrylic acid -2- methoxy acrylates, methacrylic acid -2- ethoxy ethyl esters
Oxygroup Arrcostab；The metering systems such as methacrylic acid -2- (perfluoro butyl) ethyl ester, methacrylic acid -2- (perfluoropentyl) ethyl ester
Acidic group -2- (perfluoroalkyl) ethyl ester；Benzyl acrylate；Benzyl methacrylate etc..In these, with regard to acrylic acid series polymeric compounds
Particularly preferably include acrylic acid-2-ethyl caproite, the positive fourth of acrylic acid for (methyl) acrylate compounds used in preparation
It is at least one kind of among ester, tert-butyl acrylate.In addition, (methyl) acrylate compounds can be used alone, it can also
Two or more is applied in combination with arbitrary ratio.
It is that 2nd component is included, (methyl) acrylate compounds are polymerize obtained from monomeric unit (hereinafter,
It is known as sometimes " (methyl) acrylate monomeric units ".) ratio be preferably 40 mass % or more, more preferably 50 mass %
More than, particularly preferably 60 mass % or more, furthermore it is preferred that for 95 mass % hereinafter, more preferably 90 mass % are hereinafter, especially
Preferably 85 mass % or less.By by the ratio of (methyl) acrylate monomeric units be set as the lower limiting value of above range with
On so that the heat-sensitive layer arrived and electrode active material layer (positive electrode active material layer or negative electrode active material layer),
The caking property of spacing body further increases.In addition, by the way that the ratio of (methyl) acrylate monomeric units is set as upper limit value hereinafter,
So as to obtain the temperature-sensitive layer composition of excellent in stability.
In addition, as the monomer that can be copolymerized with (methyl) acrylate compounds, can enumerate：Acrylic acid, metering system
The unsaturated carboxylic acids class such as acid, itaconic acid, fumaric acid；Ethylene glycol dimethacrylate, diethyleneglycol dimethacrylate, three
The carboxylic acid esters with 2 or more carbon-to-carbon double bonds such as hydroxymethyl-propane triacrylate；Styrene, chlorostyrene, vinyl
Toluene, t-butyl styrene, vinylbenzoic acid, vinylbenzoic acid methyl esters, vinyl naphthalene, 1-chloro-4-methyl-benzene, hydroxyl
The styrenic monomers such as Methylethyl styrene, α-methylstyrene, divinylbenzene；Acrylamide, N- methylol acryloyls
The amides such as amine, acrylamide-2-methyl propane sulfonic system monomer；Acrylonitrile, the α such as methacrylonitrile, alpha, beta-unsaturated nitriles compound；Second
Alkene, propylene etc. have the olefines of 1 carbon double bond；The diene monomers such as butadiene, isoprene；Vinyl chloride, vinylidene chloride
Equal halogen atoms monomer；The vinyl esters such as vinylacetate, vinyl propionate, butyric acid vinyl acetate, benzoic acid vinyl acetate；Methyl
The vinyl ethers such as vinyl ethers, ethyl vinyl ether, butyl vinyl ether；Methyl vinyl ketone, ethyl vinyl ketone, butyl
The vinyl ketones such as vinyl ketone, hexyl vinyl ketone, isopropenyl vinyl ketone；N-vinyl pyrrolidone, vinylpyridine
Pyridine, vinyl imidazole etc. contain heterocyclic vinyl compounds；Glycidyl acrylate, glycidyl methacrylate, allyl
Base glycidol ether etc. contains glycidyl monomer.They a variety of can be used in combination as the above-mentioned monomer that can be copolymerized.
In addition, the 2nd component can include reactive surfactant unit.Reactive surfactant unit is with general
Reactive surfactant carries out the structural unit that polymerization is formed by structure.Reactive surfactant unit constitutes the 2nd group
The part divided, and can be functioned as surfactant.
Reactive surfactant unit is the group with the polymerism that can be copolymerized with other monomers and with table
The monomer of face active group (hydrophily base and hydrophobicity base).In general, reactive surfactant has polymerism unsaturated group,
It also plays a role as hydrophobic group after the radical polymerisation.As the had polymerism unsaturated group of reactive surfactant
The example of group, can enumerate：Vinyl, allyl, ethenylidene, acrylic, isopropenyl and isobutenyl.With regard to the polymerism
It for the type of unsaturated group, can be used alone, two or more can also be applied in combination with arbitrary ratio.
In reactive surfactant, as hydrophilic part is embodied, usually there is hydrophilic radical.Reactive table
Face activating agent can be classified as the surfactant of anionic system, cationic system, nonionic system according to the type of hydrophilic radical.
The example of hydrophilic radical as anionic system can be enumerated：-SO3M ,-COOM and-PO (OH)2.It is indicated in this M
Hydrogen atom or cation.As the example of cation, can enumerate：The alkali metal ions such as lithium, sodium, potassium；The alkaline-earth metal such as calcium, magnesium from
Son；Ammonium ion；The ammonium ion of the alkylamines such as monomethyl amine, dimethylamine, monoethyl amine, triethylamine；And monoethanolamine, diethanol amine,
The ammonium ion etc. of the hydramine such as triethanolamine.
The example of hydrophilic radical as cationic system can enumerate-NH2The primary amine salts ,-NHCH such as HX3The secondary amine salts such as HX ,-
N(CH3)2The tertiary ammonium salts ,-N such as HX+(CH3)3X-Equal quaternary ammonium salts etc..X indicates halogen group herein.
The example of hydrophilic radical as nonionic system can enumerate-OH.
As the example of preferred reactive surfactant, the compound represented by following formula (I) can be enumerated.
[chemical formula 1]
In formula (I), R indicates divalent binding groups.As the example of R ,-Si-O- bases, methylene and phenylene can be enumerated.
In formula (I), R4Indicate hydrophilic radical.As R4Example ,-SO can be enumerated3NH4。
In formula (I), n indicates 1 or more and 100 integers below.
As other examples of preferred reactive surfactant, can enumerate：Ethylene oxide is gathered with having
It closes the structural unit for being formed by structure and has the structural unit that epoxy butane polymerization is formed by structure, and then in end
With the alkenyl and-SO for having terminal double bond3NH4, compound (such as polyoxyalkylene alkenyl ethers ammonium sulfate (trade name
" LATEMUL PD-104 " and " LATEMUL PD-105 ", Kao Corporation's manufacture)).
Reactive surfactant and reactive surfactant unit can be used alone, can also be arbitrarily to compare
Two or more is applied in combination in rate.
The ratio of reactive surfactant unit contained in 2nd component is preferably 0.1 mass % or more, more preferably
0.2 mass % or more, particularly preferably 0.5 mass % or more, it is then preferred that for 5 mass % hereinafter, more preferably 4 mass % with
Under, particularly preferably 2 mass % or less.
In addition, from obtain capable of being formed electrode active material layer (positive electrode active material layer or negative electrode active material layer) and
From the perspective of the temperature-sensitive layer composition of the sufficient heat-sensitive layer of adaptation of spacing body, the glass transition temperature of the 2nd component is preferred
It is -60 DEG C or more, more preferably -55 DEG C or more, further preferably -50 DEG C or more, preferably 20 DEG C hereinafter, more preferably 15
DEG C hereinafter, further preferably 10 DEG C hereinafter, be most preferably -30 DEG C or less.By the glass transition temperature of the 2nd component upper
It states in range, so as to inhibit the phenomenon that the caking property of heat-sensitive layer becomes inadequate.
Additionally, it is preferred that also maintaining the caking property for having as binder in the state that the 2nd component is divided into melting at the 1st group.
(manufacture of particle)
Particle can be for example, by carrying out the monomer for importing the 2nd component in the presence of the particle formed by the 1st component
(co) polymerization and obtain.As the monomer for importing the 2nd component is copolymerized in the presence of the particle formed by the 1st component
Method is not particularly limited, preferably in the aqueous liquid dispersion of the particle formed by the 1st component by import the 2nd component monomer into
The method of row emulsion polymerization.Thereby, it is possible to be located at the outer of the particle formed by the 1st component with obtaining the 2nd component substantial portion
Particle made of side.In addition, " (co) polymerization " refers to polymerization or copolymerization.In addition, the particle formed by the 1st component does not limit especially
It is fixed, it can be for example, by will be mixed at the 1st component, the temperature of decentralized medium and surfactant more than the fusing point of the 1st component
Afterwards, its state disperseed is made to be cooled down to prepare to be dispersed through machine.
Any one of batch type, semi continuous, continous way mode can be used as polymerization methods.In addition, polymerization pressure
Power, polymerization temperature and polymerization time are not particularly limited, and can use well known condition.
Emulsion polymerization is carried out generally according to conventional method.For example, according to " experimental chemistry lecture " volume 28, (publisher：Ball
Kind limited liability company, Japanization association compile) recorded in method carry out.I.e. following method：It is filled equipped with blender and heating
In the closed container set, water, the additives such as dispersant, emulsifier, crosslinking agent, polymerization are added in the way of as defined form
The solution of initiator and monomer, the monomer composition in stirring container make monomer etc. emulsify in water, make while stirring
Temperature rise and cause polymerization.Or following method：After so that above-mentioned monomer composition is emulsified, add it in closed container,
Similarly initiation reaction.When emulsion polymerization, commonly used surfactant in emulsion polymerization, polymerization can be used to draw
The various additives such as agent, chain-transferring agent, chelating agent, electrolyte, oxygen scavenger are sent out as polymerization auxiliary material.
Surfactant for emulsion polymerization can be lived as long as it can obtain desired particle using arbitrary surface
Property agent.As surfactant, such as neopelex, lauryl sodium sulfate, dodecyl diphenyl can be enumerated
Ether sodium disulfonate, dialkyl succinate sodium sulfonate etc..In addition, surfactant can be used alone, it can also be with arbitrary
Ratio combine uses two or more.
The amount of surfactant is arbitrary as long as it can obtain desired particle, is 100 mass parts relative to total amount
The 2nd component of importing monomer, it is more than preferably 0.5 mass parts, it is more than more preferably 1 mass parts, preferably 10 mass parts with
Under, more preferably 5 is below mass part.
In addition, when polymerisation, usually using polymerization initiator.As the polymerization initiator, as long as can it is expected
Particle can then use arbitrary polymerization initiator.As polymerization initiator, such as sodium peroxydisulfate (NaPS), over cure can be enumerated
Sour ammonium (APS), potassium peroxydisulfate (KPS) etc..Wherein preferred sodium peroxydisulfate and ammonium persulfate, more preferable ammonium persulfate.By using
Ammonium persulfate or sodium peroxydisulfate are as polymerization initiator, so as to the cycle characteristics of the lithium rechargeable battery inhibited
It reduces.
Can include molecular weight regulator or chain-transferring agent in the polymerization system in addition, in polymerization.As molecular weight
Conditioning agent or chain-transferring agent can be enumerated for example：N-hexyl mercaptan, n octylmercaptan, tert octyl mercaptan, n-dodecyl mercaptan,
The alkyl hydrosulfides such as tert-dodecylmercaotan, positive stearyl mercaptan；Dimethyl disulfide xanthate, curing diisopropyl xanthan
The xanthic acid compound such as acid esters；Terpinolene；Tetramethylthiuram disulfide, tetraethylthiuram disulfide, a vulcanization tetramethyl
The thiurams based compound such as base thiuram；The phenol based compound such as 2,6 di tert butyl 4 methyl phenol, styrenated phenol；
The allyl compounds such as allyl alcohol；The halogenated hydrocarbon compounds such as dichloromethane, methylene bromide, carbon tetrabromide；It is thioacetic acid, thio
Malic acid, 2-ethylhexyl mercaptoacetate, diphenylethlene, α-methylstyrene dimer etc..In addition, these can individually make
With a kind, two or more can also be applied in combination with arbitrary ratio.
(characteristic of temperature-sensitive layer composition)
Including the 2nd component substantial portion be located at the temperature-sensitive of particle made of the outside of the particle formed by the 1st component
Storage modulus at 60 DEG C of layer composition is 10kPa or more, preferably 100kPa or more.When the 60 of above-mentioned temperature-sensitive layer composition
DEG C when storage modulus be above range when, do not overheat extremely it is usual when bad influence will not be generated to battery behavior.
On the other hand, when the storage modulus when 60 DEG C of above-mentioned temperature-sensitive layer composition is too low, even if usual what is do not overheated extremely
Also there is the significantly reduced risk of internal resistance rising, battery performance under state.In addition, storage modulus at 60 DEG C of temperature-sensitive layer composition
Preferably 100MPa is hereinafter, more preferably 10MPa or less.
Including the 2nd component substantial portion be located at the temperature-sensitive of particle made of the outside of the particle formed by the 1st component
Storage modulus of the layer composition at 150 DEG C is 1kPa hereinafter, preferably 100Pa or less.When temperature-sensitive layer composition is at 150 DEG C
Storage modulus be above range when, can extremely overheat when so that internal resistance is fully increased.When above-mentioned temperature-sensitive layer composition exists
When storage modulus at 150 DEG C is excessive, the melting of temperature-sensitive layer composition when exception overheats becomes inadequate, when exception overheats
The rising of internal resistance becomes inadequate.In addition, storage modulus of the temperature-sensitive layer composition at 150 DEG C is preferably 1Pa or more.
Storage modulus at 60 DEG C of above-mentioned temperature-sensitive layer composition and storage modulus at 150 DEG C can pass through following surveys
Determine method and acquires.First, temperature-sensitive layer composition is dried in the state of being put into container appropriate to which film forming is
The film of thickness 0.5mm.Then, obtained film is stamped into the circle of diameter 8mm, as sample.It can use to measure and dynamically glue
The device (for example, ProductName " MCR302 ", Anton Paar companies manufacture etc.) of elasticity, is 1Hz's to the sample loading frequency
Stress, on one side with defined heating rate (such as 20 DEG C/min etc.) 25 DEG C~160 DEG C temperature range improve temperature, one
Side measures dynamic viscoelastic, and storage modulus is acquired based on the measurement result.
(lithium rechargeable battery heat-sensitive layer)
The heat-sensitive layer of the present invention is formed by temperature-sensitive layer composition, and above-mentioned temperature-sensitive layer composition includes the 2nd component essence top
Ground is divided to be located at particle made of the outside of the particle formed by the 1st component.In addition, heat-sensitive layer is preferably without using binding material
It is formed in the case of (binder) etc..Specifically, temperature-sensitive layer composition preferably only by the 2nd component substantial portion be located at by
The particle to deform when particle made of the outside for the particle that the 1st component is formed and/or heat-sensitive layer formation is formed.
Here, in a lithium ion secondary battery, anode with positive electrode active material layer and with negative electrode active material layer
Cathode usually overlapped across spacer.Moreover, the heat-sensitive layer of the present invention is preferably configured in positive electrode active material layer and bears
The opposed interlayer of pole active material layer.Specifically, the heat-sensitive layer of the present invention can be configured as the component different from spacer
Between the positive electrode active material layer and spacer of (1) anode, and/or the negative electrode active material layer of (2) cathode and spacer it
Between.In addition, the heat-sensitive layer of the present invention can configure the cathode in the positive electrode active material layer and cathode of (3) anode as spacer
Between active material layer.
It is not particularly limited as by method of the heat-sensitive layer configuration between the positive electrode active material layer and spacer of anode,
It can enumerate：Heat-sensitive layer is formed on the positive electrode active material layer of anode, it is opposed with spacer with the heat-sensitive layer formed on anode
The method that mode is overlapped；Heat-sensitive layer is formed on spacer, it is living with the anode of the heat-sensitive layer and anode that are formed on spacer
The method that the property opposed mode of material layer is overlapped；After forming heat-sensitive layer on the base material of the release properties such as peeling paper, make temperature-sensitive
Layer is removed from base material, by method etc. of the obtained heat-sensitive layer configuration between the positive electrode active material layer and spacer of anode.
In addition, as method of the heat-sensitive layer configuration between the negative electrode active material layer and spacer of cathode is not special
Limitation, can enumerate：Heat-sensitive layer is formed on the negative electrode active material layer of cathode, with heat-sensitive layer and the spacer pair formed on cathode
The method that the mode set is overlapped；Heat-sensitive layer is formed on spacer, with the negative of the heat-sensitive layer that is formed on spacer and cathode
The method that active material layer opposed mode in pole is overlapped；After heat-sensitive layer being formed on the base material of the release property of peeling paper etc.,
So that heat-sensitive layer is removed from base material, obtained heat-sensitive layer is configured into the method between the negative electrode active material layer and spacer of cathode
Deng.
In addition, as using heat-sensitive layer as spacer arrangement anode positive electrode active material layer and cathode negative electrode active
Method between material layer is not particularly limited, and can enumerate after forming heat-sensitive layer on the base material of the release properties such as peeling paper, make heat
Photosensitive layer is removed from base material, and obtained heat-sensitive layer is configured the negative electrode active material layer in the positive electrode active material layer and cathode of anode
Between method etc..In addition, can also enumerate：Heat-sensitive layer is formed on the positive electrode active material layer of anode, with what is formed on anode
The heat-sensitive layer mode opposed with the negative electrode active material layer of cathode overlaps the method for positive electrode and negative electrode, the negative electrode active material in cathode
Heat-sensitive layer is formed on matter layer, is overlapped just in such a way that the heat-sensitive layer formed on cathode is opposed with the positive electrode active material layer of anode
The method of pole and cathode.
Here, being configured between the positive electrode active material layer and spacer of above-mentioned (1) anode, (2) cathode by heat-sensitive layer
Negative electrode active material layer and spacer between, the negative electrode active material layer of the positive electrode active material layer of (3) anode and cathode it
Between method in, the forming method of heat-sensitive layer is not particularly limited.Such as it can be by using doctor blade method, infusion process, inverse
Tumbler coating, direct roll coating process, gravure method, extrusion, the direct rubbing method of comma roller, die coating method, slip rubbing method, spread coating etc.
On positive electrode active material layer, on negative electrode active material layer, on spacer or on the base material of release property coating include heat-sensitive layer group
The paste compound for closing object, makes the paste compound of coating dry, to form heat-sensitive layer.
As drying means, it can enumerate and for example utilize warm air, hot wind, the seasoning of low wet wind, boulton process, utilization
The seasoning of the irradiations such as (remote) infrared ray, electron beam.Wherein, preferably by the seasoning of hot wind, utilize the irradiation of far infrared
Seasoning.
Drying time is usually 1~60 minute.In addition, drying temperature is usually the fusing point of 40 DEG C or more and the 1st component of ratio
Low temperature.It can be by will include that being coated and dried for paste compound of temperature-sensitive layer composition is repeated a number of times to shape
At heat-sensitive layer.Furthermore, it is possible to further be heated as needed after heat-sensitive layer is formed.
Here, the paste compound comprising temperature-sensitive layer composition can by mix above-mentioned particle, water equal solvent etc. with
And arbitrary additive is to obtain.
From obtain with electrode active material layer (positive electrode active material layer or negative electrode active material layer), spacer it is good
The viewpoint of adaptation and from obtain the state not overheated extremely it is usual when for low-resistance lithium rechargeable battery
Viewpoint is set out, the thickness of heat-sensitive layer be preferably 0.1 μm or more and 5 μm hereinafter, more preferably 0.2 μm or more and 4 μm hereinafter, into one
Preferably 0.3 μm or more and 3 μm or less of step.
In addition, for temperature-sensitive layer composition, from the heat-sensitive layer made and electrode active material layer (positive active material
Layer or negative electrode active material layer), from the perspective of the adaptation of spacer further increases, preferably indicate temperature-sensitive layer composition
The value of adaptation is 1 or more.In addition, indicating that the value of the adaptation of temperature-sensitive layer composition refers to by carrying out JIS at 25 DEG C
Initial stage cohesion test (angle of inclination is 20 °) ball number obtained from of Z0237 defineds.
(lithium rechargeable battery)
The heat-sensitive layer of the present invention can be used for lithium rechargeable battery.Here, in the present invention, lithium rechargeable battery includes
Anode, cathode, spacer, heat-sensitive layer and electrolyte.In addition, heat-sensitive layer can will be used own as spacer, in the feelings
Under condition, lithium ion battery includes anode, cathode, heat-sensitive layer and electrolyte.
(anode)
The positive positive electrode active material layer that usually there is collector and formed on a current collector.Moreover, anode is without spy
It does not limit, can make to be formed by known method.Specifically, anode can be obtained for example, by following methods：It will
Including positive active material, binding material, solvent, as needed the anode sizing agent group of conductive material and thickener for using etc.
It closes object coating on a current collector, keeps the anode paste compound of coating dry and form positive electrode active material layer.In addition, being formed
Positive electrode active material layer can further carry out as needed heat treatment and/or pressurized treatments.Moreover, as positive-active
Substance, binding material, solvent and conductive material and thickener as needed and use are not particularly limited, and can use
Various positive active materials, binding material, solvent, conductive material and the thickener that can be used in lithium rechargeable battery.
(cathode)
Cathode is usually with collector and the negative electrode active material layer formed on a current collector.Moreover, cathode is without spy
It does not limit, can make to be formed by known method.Specifically, cathode can be obtained for example, by following methods：It will
Including negative electrode active material, binding material, solvent, as needed the negative electrode slurry group of conductive material and thickener for using etc.
It closes object coating on a current collector, keeps the negative electrode slurry composition of coating dry and form negative electrode active material layer.In addition, being formed
Negative electrode active material layer can further carry out as needed heat treatment and/or pressurized treatments.Moreover, as negative electrode active
Substance, binding material, solvent and conductive material and thickener as needed and use are not particularly limited, and can use
Various negative electrode active materials, binding material, solvent, conductive material and the thickener that can be used in lithium rechargeable battery.
(spacer)
In the present invention, it can be used using heat-sensitive layer as spacer.As not used heat-sensitive layer as spacer
In the case of spacer, can use for example：Including the vistanexes such as polyethylene, polypropylene, aromatic polyamide resin
Microporous barrier or non-woven fabrics, include the Porous resinous coat etc. of inorganic ceramic powder.
Moreover, in the case where not using heat-sensitive layer as spacer, the heat resisting temperature of spacer is preferably than in temperature-sensitive
The fusing point of 1st component of the particle used in layer is high.
The behaviour when resistance based on spacer out of lithium rechargeable battery becomes smaller and manufactures lithium rechargeable battery
From the perspective of the property made is excellent, the thickness of spacer is preferably 0.5 μm or more and 40 μm hereinafter, more preferably 1 μm or more and 30 μ
M is hereinafter, further preferably 1 μm or more and 25 μm or less.
(electrolyte)
Electrolyte is not particularly limited, and can use for example will be dissolved in the molten of non-water system as the lithium salts of supporting electrolyte
Electrolyte in agent.As lithium salts, can enumerate for example：LiPF6、LiAsF6、LiBF4、LiSbF6、LiAlCl4、LiClO4、
CF3SO3Li、C4F9SO3Li、CF3COOLi、(CF3CO)2NLi、(CF3SO2)2NLi、(C2F5SO2) NLi etc..It is preferable to use especially easily
In being dissolved in the LiPF for showing high dissociation degree in solvent6、LiClO4、CF3SO3Li.These individually or can mix two or more and make
With.Relative to electrolyte, the amount of supporting electrolyte is usually 1 mass % or more, and preferably 5 mass % or more are usually in addition
30 mass % are hereinafter, preferably 20 mass % or less.When the amount of supporting electrolyte is above range, ionic conductance can be inhibited
Degree decline and the charge characteristic of battery, flash-over characteristic decline the phenomenon that.
As the solvent used in the electrolytic solution, as long as the solvent that supporting electrolyte dissolves is made to be not particularly limited,
Usually it can be used：Dimethyl carbonate (DMC), ethylene carbonate (EC), diethyl carbonate (DEC), propene carbonate (PC), carbonic acid
The alkyl carbonates esters such as butene esters (BC) and methyl ethyl carbonate (MEC)；The esters such as gamma-butyrolacton, methyl formate；1,2- bis-
The ethers such as Ethyl Methyl Ether and tetrahydrofuran；The sulfur-containing compounds class such as sulfolane and dimethyl sulfoxide (DMSO).Especially since easily
In obtaining, high ionic conductance, use temperature range are extensive, therefore preferably dimethyl carbonate, ethylene carbonate, propylene carbonate
Ester, diethyl carbonate, methyl ethyl carbonate.These can be independent or mix two or more use.Additionally it is possible to make in electrolyte
It is used containing additive.In addition, as additive, the preferred compound of the carbonic esters system such as vinylene carbonate (VC).
As electrolyte other than the above, can enumerate：So that electrolyte is contained and is immersed in the polymerizations such as polyethylene oxide, polyacrylonitrile
Gel-like polymer electrolyte in object electrolyte, lithium sulfide, LiI, Li3N、Li2S-P2S5The inorganic solid electrolytes such as glass ceramics
Matter.
Lithium rechargeable battery is obtained by following methods：It is living to be located at anode opposite one another with the heat-sensitive layer of the present invention
Mode between property material layer and negative electrode active material layer folds cathode, anode and heat-sensitive layer across optional spacer
It closes, crimp, folded according to cell shapes etc. and be put into battery case, injection electrolyte is sealed in battery case
Mouthful.That is, lithium rechargeable battery has：Anode with positive electrode active material layer opposed with positive electrode active material layer has
The cathode of negative electrode active material layer and configuration are between positive electrode active material layer and negative electrode active material layer opposite one another
Heat-sensitive layer.In turn, it is anti-excessively electric also can be put into porous metal mesh, fuse, PTC element etc. as needed for lithium rechargeable battery
Fluid element, guide plate etc. prevent the pressure of inside battery from rising, cross charge and discharge.The shape of battery can be layer-built battery type, coin
Type, coin shape, piece type, cylinder type, rectangular, platypelloid type etc. are any.
Moreover, lithium rechargeable battery heat-sensitive layer according to the present invention, by making inside battery when overheating extremely
Resistance rises, and hinders temperature rise so as to effectively reduce electric current.
Embodiment
Hereinafter, enumerating, examples illustrate the present invention, but the present invention not due to these embodiments by any limit
It is fixed.In addition, unless otherwise specified, " part " and " % " of the present embodiment is respectively " mass parts " and " quality % ".Each physics
The measurement and evaluation of property and characteristic are carried out by the following method.
<The measurement of fusing point>
For the particle formed by the 1st component used in embodiment and comparative example, fusing point is measured as following.
Using differential scanning type calorimeter (Nanotechnology is manufactured, DSC6220SII), it is based on JIS K7121
(1987), after sample (particle formed by the 1st component) being heated to 30 DEG C higher than fusing point or more of temperature, with cooling velocity-
10 DEG C/min are cooled to room temperature, then with heating rate 10 DEG C/min be measured.
<The measurement of molecular weight>
For the polyolefin used in embodiment and comparative example, number-average molecular weight is measured as following.
First, 5mL solvents are added in 10mg samples (polyolefin), stirs 30 minutes and is dissolved at 140~150 DEG C.
Then, the solution is filtered using 0.5 μm of filter, as measurement sample.The measurement sample is used into gel permeation chromatography
(GPC) it is analyzed under the following conditions, number-average molecular weight is acquired according to analysis result.
Measurement device：PL-220 (Polymer Laboratories manufactures)
Column：Shodex HT-G, HT-806M (1), HT-803 (1) (diameter 8.0mm × 30cm, Showa electrician manufacture)
Solvent：Trichloro-benzenes+0.1%BHT
Flow velocity：1.0mL/ minute
Detector：Differential refractive index detector RI
Column temperature：145℃
Primary standard substance：Monodisperse polystyrene (Tosoh manufactures)
<The measurement of glass transition temperature>
The glass transition temperature of 2nd component (is measured and is tried by polymer of the preparation with composition identical with the 2nd component
Sample) and be measured.Specifically, the monomer of the 2nd component of importing used in preparation using the 2nd component, with the 2nd component
The identical polymerizing condition of polymerizing condition under prepare become measure sample polymer, use differential scanning type calorimeter
(Nanotechnology is manufactured, DSC6220SII), based on JIS K7121 (1987) to the glass transition temperature of measurement sample
It is measured, the glass transition temperature as the 2nd component.
<The measurement of storage modulus>
Make the temperature-sensitive layer composition aqueous dispersions prepared in embodiment and comparative example in the drying 168 hours of 23 DEG C of temperature, system
At the film of thickness 0.5mm, it is stamped into the circle of a diameter of 8mm, as measurement sample.Then, using following devices, following
Under conditions of measure dynamic viscoelastic, storage modulus when acquiring 60 DEG C and 150 DEG C based on the measurement result.
Device：Rheometer MCR302 (Anton Paar manufactures)
Set temperature range：25 DEG C~160 DEG C
Set heating rate：20 DEG C/min
Measurinng frequency：1Hz
<The adaptation of heat-sensitive layer>
On the PET film through sided corona treatment by the temperature-sensitive layer composition moisture dispersion liquid prepared in embodiment and comparative example into
Row coating is dry and forms the composition layer of 2 μm of thickness, as measurement sample.Based on JIS Z0237, in 23 DEG C of environment of temperature
Under, by said determination sample in such a way that composition layer becomes surface with angle of inclination 20 ° configure, by diameter from 1/32 English
The steel ball of very little to 32/32 inch of 30 kinds of sizes is tumbled with initial velocity 0 from the position of the top 10cm on inclined-plane.It will be on combination layer
Value of the size (ball number) of the ball of the maximum gauge of stopping as the adaptation for indicating heat-sensitive layer, is commented with benchmark below
Valence.If the value is the range of " qualification ", then it represents that be the heat-sensitive layer of excellent adhesion.
It is qualified：Ball number is 1 or more
It is unqualified：Ball number is 0
<Resistance when abnormal overheat is ascending>
By the lithium rechargeable battery made in embodiment and comparative example in the environment of temperature is 60 DEG C, using 1C, (C is volume
Numerical value represented by constant volume (mA)/1h (time)) it is charged to the 50% of depth of charge (SOC), in being then with the 50% of SOC
The heart carries out charging in 10 seconds respectively with 0.5C, 1.0C, 1.5C, 2.0C and 10 seconds discharge.Then, by the battery after 10 seconds of discharge side
Voltage charts relative to current value, is acquired using its slope as IV resistance (Ω) (IV resistance when electric discharge).In addition, will
(using the IV resistance of the lithium rechargeable battery of 160 DEG C of heating cathodes (A3))/(using the lithium of not 160 DEG C of heating cathodes (A2)
The IV resistance of ion secondary battery) } × 100 (%) value as IV resistance climbings, evaluated with benchmark below.The value
Higher, resistance when indicating abnormal overheat is ascending more excellent.
A：IV resistance climbings are 400% or more
B：IV resistance climbings are 300% less than 400%
C：IV resistance climbings are 200% less than 300%
D：IV resistance climbings are less than 200%
(embodiment 1)
<The preparation of temperature-sensitive layer composition (A1) aqueous dispersions>
Be added in polymerization tank A 100 parts of ion exchange water, be calculated as using solid constituent a great deal of 100 parts as the 1st group
30% water-based emulsion of the polyolefin (polyethylene-based wax (fusing point is 95 DEG C, number-average molecular weight 7300)) divided, and then it is added 0.2
The ammonium persulfate of part is heated to 70 DEG C as polymerization initiator and 10 parts of ion exchange waters.In addition, in other polymerization tank B
It is middle be added 30 parts ion exchange water, as import the 2nd component monomer 35 parts of 2-EHA (below sometimes
Referred to as " 2-EHA ".) and 15 parts of styrene (hereinafter sometimes referred to " St ".) in turn, 0.5 part of ethylene glycol dimethyl third is added
Olefin(e) acid ester, be calculated as with solid constituent a great deal of 2 parts polyoxyalkylene alkenyl ether ammonium sulfate 20% aqueous solution, be sufficiently stirred, go through
When be added continuously in polymerization tank A within 120 minutes.In turn, continue polymerisation while maintaining 70 DEG C until polymerization turns
Rate reaches 98%.It cools down and terminates reaction, obtain the aqueous dispersions of temperature-sensitive layer composition (A1).
In addition, the glass transition temperature for constituting the 2nd component of the particle in obtained temperature-sensitive layer composition (A1) is -37
℃.In particle in the temperature-sensitive layer composition (A1), it is located at the particle formed by the 1st component to the 2nd component substantial portion
Outside.In addition, storage modulus at 60 DEG C of obtained temperature-sensitive layer composition (A1) is 204kPa, energy storage mould at 150 DEG C
Amount is 70Pa, indicates that the value (ball number) of the adaptation of heat-sensitive layer is 1.
<The making of lithium ion secondary battery anode (positive (A2) and 160 DEG C of heating cathodes (A3))>
It will in such a way that solid constituent is calculated as 90: 5: 5 by the mass ratio of positive active material, binding material and conductive material
Cobalt acid lithium (LiCoO as a positive electrode active material2；Number average bead diameter：20 μm), as the dissolving of binding material gather inclined difluoro second
The n-methyl-2-pyrrolidone solution of alkene is mixed as the acetylene carbon black of conductive material, makes anode slurry compositions
Object.After using paste compound to be coated on as on the aluminium foil of collector at anode, at 80 DEG C, then it is dried at 140 DEG C.So
Rolled to form positive electrode active material layer by using stack afterwards.Then, temperature-sensitive layer composition (A1) is water-dispersed
Liquid is coated on positive electrode active material layer, is then dried in the temperature of the fusing point less than the 1st component, in positive active material
Heat-sensitive layer is formed on layer.Then, collector lug is installed, is thus made multiple positive (A2).In turn, to a part for the anode
5 minutes are heated in 160 DEG C under vacuum conditions to make 160 DEG C of heating cathodes (A3).
<The making of lithium ion secondary battery cathode>
It will be made in such a way that solid constituent is calculated as 100: 2: 2 by the mass ratio of negative electrode active material, thickener and binder
For the artificial graphite (volume average particle size of negative electrode active material：25 μm), as thickener sanlose water
Solution and the aqueous dispersions of styrene-butadiene copolymer as binding material are mixed, and negative paste combination is made
Object.Negative electrode slurry composition is coated on the copper foil as collector, then at 60 DEG C, is then dried at 120 DEG C.
Then rolled using stack, collector lug is installed and makes cathode.
<The making of electrolyte>
By ethylene carbonate and diethyl carbonate with mass ratio for 1：In the solvent that 2 mode is mixed, to become
The mode of 1.0M dissolves the LiPF as solute6And make electrolyte.
<The making of lithium rechargeable battery>
Make the spacer of polyethylene be inserted into making lithium ion secondary battery anode with heat-sensitive layer and lithium from
Between sub- secondary battery cathode, in such a way that the positive electrode active material layer and the negative electrode active material layer with heat-sensitive layer is opposed into
Row winds and makes coiling body, is compressed from a direction.Compressed coiling body is to overlook ellipse.This is compressed
Coiling body and electrolyte are enclosed together in defined aluminium layer drawn-shell case, and the lithium ion two that quota capacity is 720mAh is thus made
Primary cell.In addition, as lithium ion secondary battery anode, positive (A2) and 160 DEG C of heating cathodes (A3) is used to make respectively
Lithium rechargeable battery, resistance when evaluating abnormal overheat are ascending.The results are shown in Table 1.
(embodiment 2)
The type of the 1st component used in the preparation of temperature-sensitive layer composition (A1) aqueous dispersions is changed to polyethylene-based
Wax (fusing point is 130 DEG C, molecular weight 9900), in addition to this, prepares temperature-sensitive layer composition (A1) moisture similarly to Example 1
Dispersion liquid.In particle in the temperature-sensitive layer composition (A1), it is located at the grain formed by the 1st component to the 2nd component substantial portion
The outside of son.In addition, storage modulus at 60 DEG C of obtained temperature-sensitive layer composition (A1) is 2010kPa, energy storage at 150 DEG C
Modulus is 80Pa, indicates that the value (ball number) of the adaptation of heat-sensitive layer is 1.Using temperature-sensitive layer composition (A1) obtained above, remove
Except this, lithium ion secondary battery anode (positive (A2) and 160 DEG C of heating cathodes (A3)) is carried out similarly to Example 1
Making, the making of lithium ion secondary battery cathode, the making of electrolyte and lithium rechargeable battery making.Then with implementation
Example 1 is carried out similarly evaluation.The results are shown in Table 1.
(embodiment 3)
As the monomer of the 2nd component of importing used in the preparation of temperature-sensitive layer composition (A1) aqueous dispersions, 35 are used
The n-butyl acrylate (hereinafter sometimes referred to " BA " of part.) and 15 parts of acrylonitrile (hereinafter sometimes referred to " AN ".), except this with
Outside, temperature-sensitive layer composition (A1) aqueous dispersions are prepared similarly to Example 1.Particle in the temperature-sensitive layer composition (A1)
In, the 2nd component substantial portion it is located at the outside of the particle formed by the 1st component.In addition, obtained temperature-sensitive layer composition
(A1) glass transition temperature of the 2nd component is -20 DEG C.In addition, storage modulus at 60 DEG C of temperature-sensitive layer composition (A1)
For 268kPa, storage modulus at 150 DEG C is 70Pa, indicates that the value (ball number) of the adaptation of heat-sensitive layer is 1.It is obtained using above-mentioned
Temperature-sensitive layer composition (A1) in addition to this carry out lithium ion secondary battery anode (positive (A2) similarly to Example 1
With 160 DEG C of heating cathodes (A3)) making, the making of lithium ion secondary battery cathode, the making of electrolyte and lithium ion two
The making of primary cell.Then it is evaluated similarly to Example 1.The results are shown in Table 1.
(comparative example 1)
The type of the 1st component used in the preparation of temperature-sensitive layer composition (A1) aqueous dispersions is changed to polyethylene-based
Wax (fusing point is 50 DEG C, molecular weight 4500), in addition to this, prepares temperature-sensitive layer composition (A1) moisture similarly to Example 1
Dispersion liquid.In particle in the temperature-sensitive layer composition (A1), it is located at the grain formed by the 1st component to the 2nd component substantial portion
The outside of son.In addition, storage modulus at 60 DEG C of obtained temperature-sensitive layer composition (A1) is 150Pa, energy storage mould at 150 DEG C
Amount is 70Pa, indicates that the value (ball number) of the adaptation of heat-sensitive layer is 1.Using temperature-sensitive layer composition (A1) obtained above, this is removed
Except, the system of lithium ion secondary battery anode (positive (A2) and 160 DEG C of heating cathodes (A3)) is carried out similarly to Example 1
Work, the making of lithium ion secondary battery cathode, the making of electrolyte and lithium rechargeable battery making.Then with embodiment
1 is carried out similarly evaluation.The results are shown in Table 1.
(comparative example 2)
As the monomer of the 2nd component of importing used in the preparation of temperature-sensitive layer composition (A1) aqueous dispersions, 70 are used
2-EHA and 30 part of the St of part prepares temperature-sensitive layer composition (A1) aqueous dispersions similarly to Example 1 in addition to this.At this
In particle in temperature-sensitive layer composition (A1), the outside of the 2nd component coating particle formed by the 1st component completely.In addition, obtaining
60 DEG C of temperature-sensitive layer composition (A1) when storage modulus be 1490kPa, storage modulus at 150 DEG C is 70kPa, indicates heat
The value (ball number) of the adaptation of photosensitive layer is 1.It is in addition to this, same with embodiment 1 using temperature-sensitive layer composition (A1) obtained above
Carry out to sample making, the lithium ion secondary electricity of lithium ion secondary battery anode (positive (A2) and 160 DEG C of heating cathodes (A3))
The making of pond cathode, the making of electrolyte and lithium rechargeable battery making.Then it is commented similarly to Example 1
Valence.The results are shown in Table 1.
(comparative example 3)
Be added without the 2nd component, by be added 100 parts of ion exchange water, be calculated as using solid constituent a great deal of 100 parts as
The mixture of 30% water-based emulsion of the polyethylene-based wax (fusing point is 95 DEG C, number-average molecular weight 7300) of the 1st component is as warm
Photosensitive layer composition (A1) aqueous dispersions.In addition, in particle in the temperature-sensitive layer composition (A1), the 2nd component both not quilt completely
The outside of the particle formed by the 1st component is covered, the outside of the particle formed by the 1st component is also located to non-substantial portion.This
Outside, storage modulus at 60 DEG C of the temperature-sensitive layer composition (A1) obtained is 172kPa, and storage modulus at 150 DEG C is 70Pa,
Indicate that the value (ball number) of the adaptation of heat-sensitive layer is 0.Using temperature-sensitive layer composition (A1) obtained above, similarly to Example 1
Ground carries out the making of lithium ion secondary battery anode (positive (A2) and 160 DEG C of heating cathodes (A3)), but temperature-sensitive layer composition
(A1) adaptation is insufficient, cannot form heat-sensitive layer.It is thus impossible to carry out the making of lithium rechargeable battery, cannot carry out
The ascending evaluation of resistance when abnormal overheat.
[table 1]
As shown in table 1, lithium rechargeable battery is formed with heat-sensitive layer by temperature-sensitive layer composition, above-mentioned temperature-sensitive layer composition packet
It is located at particle made of the outside of the particle formed by the 1st component containing the 2nd component substantial portion, above-mentioned temperature-sensitive at 60 DEG C
The storage modulus of layer composition is 10kPa or more, the storage modulus of above-mentioned temperature-sensitive layer composition at 150 DEG C be 1kPa hereinafter,
The adaptation of the lithium rechargeable battery heat-sensitive layer is good, uses the abnormal mistake of lithium rechargeable battery made of the heat-sensitive layer
Resistance when hot is ascending also good.
Claims (6)
1. a kind of lithium rechargeable battery heat-sensitive layer, is formed by temperature-sensitive layer composition, above-mentioned temperature-sensitive layer composition includes the 2nd group
It is located at particle made of the outside of the particle formed by the 1st component with dividing substantial portion,
The storage modulus of temperature-sensitive layer composition at 60 DEG C is 10kPa or more,
The storage modulus of temperature-sensitive layer composition at 150 DEG C is 1kPa or less.
2. lithium rechargeable battery heat-sensitive layer according to claim 1 is configured in positive electrode active material opposite one another
Between matter layer and negative electrode active material layer.
3. lithium rechargeable battery heat-sensitive layer according to claim 1 or 2, wherein the fusing point of the 1st component is 60
DEG C or more and 160 DEG C or less.
4. lithium rechargeable battery heat-sensitive layer described in any one of claim 1 to 3, wherein the 2nd component
Glass transition temperature is -60 DEG C or more and 20 DEG C or less.
5. lithium rechargeable battery heat-sensitive layer according to any one of claims 1 to 4, the 1st component includes number
Average molecular weight is 5000 or more and 15000 polyolefin below.
6. a kind of lithium rechargeable battery has power between the positive electrode active material layer and the negative electrode active material layer opposite one another
Lithium rechargeable battery heat-sensitive layer described in any one of sharp claim 1~5.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2015-256592 | 2015-12-28 | ||
| JP2015256592 | 2015-12-28 | ||
| PCT/JP2016/087117 WO2017115647A1 (en) | 2015-12-28 | 2016-12-13 | Heat-sensitive layer for lithium ion secondary batteries |
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| Publication Number | Publication Date |
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| CN108475749A true CN108475749A (en) | 2018-08-31 |
| CN108475749B CN108475749B (en) | 2020-10-30 |
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|---|---|
| US (1) | US10651447B2 (en) |
| EP (1) | EP3399572B1 (en) |
| JP (1) | JP6798505B2 (en) |
| KR (1) | KR102628821B1 (en) |
| CN (1) | CN108475749B (en) |
| HU (1) | HUE059953T2 (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111200101A (en) * | 2018-11-16 | 2020-05-26 | 宁德时代新能源科技股份有限公司 | Positive pole piece and electrochemical device |
| CN113764613A (en) * | 2020-05-29 | 2021-12-07 | 珠海冠宇电池股份有限公司 | Multilayer composite positive pole piece and secondary battery containing same |
| CN113764612A (en) * | 2020-05-29 | 2021-12-07 | 珠海冠宇电池股份有限公司 | Positive pole piece containing high-safety thermosensitive coating and lithium ion battery |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| KR20210039372A (en) | 2018-08-07 | 2021-04-09 | 니폰 제온 가부시키가이샤 | Composition for non-aqueous secondary battery functional layer and its manufacturing method, functional layer for non-aqueous secondary battery, non-aqueous secondary battery member, and non-aqueous secondary battery |
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| CN111200101A (en) * | 2018-11-16 | 2020-05-26 | 宁德时代新能源科技股份有限公司 | Positive pole piece and electrochemical device |
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| CN113764612A (en) * | 2020-05-29 | 2021-12-07 | 珠海冠宇电池股份有限公司 | Positive pole piece containing high-safety thermosensitive coating and lithium ion battery |
Also Published As
| Publication number | Publication date |
|---|---|
| US20190165350A1 (en) | 2019-05-30 |
| CN108475749B (en) | 2020-10-30 |
| US10651447B2 (en) | 2020-05-12 |
| JP6798505B2 (en) | 2020-12-09 |
| PL3399572T3 (en) | 2022-11-21 |
| KR102628821B1 (en) | 2024-01-23 |
| EP3399572A1 (en) | 2018-11-07 |
| KR20180091018A (en) | 2018-08-14 |
| EP3399572B1 (en) | 2022-08-10 |
| EP3399572A4 (en) | 2019-06-19 |
| HUE059953T2 (en) | 2023-01-28 |
| JPWO2017115647A1 (en) | 2018-10-18 |
| WO2017115647A1 (en) | 2017-07-06 |
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